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Liquid chromatographic enantioseparation of several amino acids as nitrobenzoxadiazole derivatives on polysaccharide trisphenylcarbamate derived chiral stationary phases

  • Suraj Adhikari;Alisha Bhandari;Wonjae Lee
    • Analytical Science and Technology
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    • v.36 no.4
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    • pp.143-151
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    • 2023
  • Considering the greater role of α-amino acids in our daily lives, the enantiomer resolution of seven α-amino acids derivatized with fluorogenic reagent (4-fluoro-7-nitro-2,1,3-benzoxadiazole, NBD-F) by chiral HPLC on amylose or cellulose trisphenylcarbamate derived chiral stationary phases (CSPs) under simultaneous ultraviolet (UV) and fluorescence (FL) detection was performed. The degree of enantioseparation and resolution was affected by nature and selector backbones of the CSPs as well as the kind of amino acids. Baseline enantiomer separation and resolutions were observed for the enantiomers of all analytes as NBD derivatives especially on coated type amylose tris(3,5-dimethylphenylcarbamate) derived CSPs (Chiralpak AD-H and Lux Amylose-1). The other CSPs also showed good enantioselectivity except for the CSPs (Chiralpak IB, Chiralcel OD-H and Lux Cellulose-1) having cellulose tris(3,5-dimethylphenylcarbamate) as chiral selectors. The developed analytical chiral method was applied to determine the enantiomeric purity of seven commercially available L-α-amino acids and the impurities as D-forms were found to be in the range 0.08-0.87 %, respectively. The intra- and interday accuracy and precision assays showed high accuracy and precision of the developed analytical method. This chiral HPLC method for the enantiomer resolution of amino acids using fluorescent derivatization could be useful for the determination of enantiomeric purity of pharmaceuticals and biological study for amino acid type compounds among chiral drugs.

Ebert-Fastie spectrograph using the Transformable Reflective Telescope kit

  • Ahn, Hojae;Mo, Gyuchan;Jung, Hyeonwoo;Choi, Junwhan;Kwon, Dou Yoon;Lee, Minseon;Kim, Dohoon;Lee, Sumin;Park, Woojin;Lee, Ho;Park, Kiehyun;Kim, Hyunjong;Pak, Soojong
    • The Bulletin of The Korean Astronomical Society
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    • v.45 no.1
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    • pp.40.4-40.4
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    • 2020
  • Kyung Hee university invented the Transformable Reflective Telescope (TRT) for optical experiment and education. The TRT kit can transform into three optical configurations from Newtonian to Cassegrain to Gregorian by exchanging the secondary mirror. We designed the Ebert-Fastie spectrograph as an extension of the TRT kit. The primary mirror of the TRT kit serves as both collimator and camera lens, and the reflective grating as the dispersing element is placed along the optical axis of the primary mirror. We designed and fabricated the grating holder and the source units using 3D printer. Baffle was also fabricated to suppress the stray light, which was reduced by 83%. The spectrograph can observe the optical wavelength range (4000Å~7000Å). Measured resolving power (R=λ/Δλ) was ~700 with slit width of 0.18mm. The spectrograph is optimized for f/24, and the spectral pixel scale is 0.49Å/pixel with Canon 550D detector. We present the sample spectra of discharged Ne, Ar and Kr gases. The flexible setting and high performance make this spectrograph a useful tool for education and experiment.

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Determination of N-nitrosodimethylamine in zidovudine using high performance liquid chromatography-tandem mass spectrometry

  • Yujin Lim;Aelim Kim;Yong-Moon Lee;Hwangeui Cho
    • Analytical Science and Technology
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    • v.36 no.6
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    • pp.281-290
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    • 2023
  • Zidovudine is an antiretroviral agent prescribed for the prevention and treatment of human immunodeficiency virus/acquired immune deficiency syndrome (HIV/AIDS). It is typically recommended to be used in combination with other antiretroviral drugs. Zidovudine has the potential to generate N-nitrosodimethylamine (NDMA) in the presence of dimethylamine and nitrite salt under acidic reaction conditions during the drug manufacturing process. NDMA is a potent human carcinogen that may be detected in drug substances or drug products. An analytical method was developed to determine NDMA in pharmaceuticals including zidovudine using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The analysis involved reversed-phase chromatography on a Kinetex F5 column with a mobile phase comprising water-acetonitrile mixtures. The detection of positively charged ions was conducted using atmospheric pressure chemical ionization (APCI). The calibration curve demonstrated excellent linearity (r = 0.9997) across the range of 1-50 ng/mL with a highly sensitive limit of detection (LOD) at 0.3 ng/mL. The developed method underwent thorough validation for specificity, linearity, accuracy, precision, robustness, and system suitability. This sensitive and specific analytical method was applied for detecting NDMA in zidovudine drug substance and its formulation currently available in the market, indicating its suitability for drug quality management purposes.

Potential of multispectral imaging for maturity classification and recognition of oriental melon

  • Seongmin Lee;Kyoung-Chul Kim;Kangjin Lee;Jinhwan Ryu;Youngki Hong;Byeong-Hyo Cho
    • Korean Journal of Agricultural Science
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    • v.50 no.3
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    • pp.485-496
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    • 2023
  • In this study, we aimed to apply multispectral imaging (713 - 920 nm, 10 bands) for maturity classification and recognition of oriental melons grown in hydroponic greenhouses. A total of 20 oriental melons were selected, and time series multispectral imaging of oriental melons was 7 - 9 times for each sample from April 21, 2023, to May 12, 2023. We used several approaches, such as Savitzky-Golay (SG), standard normal variate (SNV), and Combination of SG and SNV (SG + SNV), for pre-processing the multispectral data. As a result, 713 - 759 nm bands were preprocessed with SG for the maturity classification of oriental melons. Additionally, a Light Gradient Boosting Machine (LightGBM) was used to train the recognition model for oriental melon. R2 of recognition model were 0.92, 0.91 for the training and validation sets, respectively, and the F-scores were 96.6 and 79.4% for the training and testing sets, respectively. Therefore, multispectral imaging in the range of 713 - 920 nm can be used to classify oriental melons maturity and recognize their fruits.

Design and Fabrication of the 0.1${\mu}{\textrm}{m}$ Г-Shaped Gate PHEMT`s for Millimeter-Waves

  • Lee, Seong-Dae;Kim, Sung-Chan;Lee, Bok-Hyoung;Sul, Woo-Suk;Lim, Byeong-Ok;Dan-An;Yoon, yong-soon;kim, Sam-Dong;Shin, Dong-Hoon;Rhee, Jin-koo
    • Journal of electromagnetic engineering and science
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    • v.1 no.1
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    • pp.73-77
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    • 2001
  • We studied the fabrication of GaAs-based pseudomorphic high electron mobility transistors(PHEMT`s) for the purpose of millimeter- wave applications. To fabricate the high performance GaAs-based PHEMT`s, we performed the simulation to analyze the designed epitaxial-structures. Each unit processes, such as 0.1 m$\mu$$\Gamma$-gate lithography, silicon nitride passivation and air-bridge process were developed to achieve high performance device characteristics. The DC characteristics of the PHEMT`s were measured at a 70 $\mu$m unit gate width of 2 gate fingers, and showed a good pinch-off property ($V_p$= -1.75 V) and a drain-source saturation current density ($I_{dss}$) of 450 mA/mm. Maximum extrinsic transconductance $(g_m)$ was 363.6 mS/mm at $V_{gs}$ = -0.7 V, $V_{ds}$ = 1.5 V, and $I_{ds}$ =0.5 $I_{dss}$. The RF measurements were performed in the frequency range of 1.0~50 GHz. For this measurement, the drain and gate voltage were 1.5 V and -0.7 V, respectively. At 50 GHz, 9.2 dB of maximum stable gain (MSG) and 3.2 dB of $S_{21}$ gain were obtained, respectively. A current gain cut-off frequency $(f_T)$ of 106 GHz and a maximum frequency of oscillation $(f_{max})$ of 160 GHz were achieved from the fabricated PHEMT\\`s of 0.1 m$\mu$ gate length.h.

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Reduction in Residual Pesticides and Quercetin Yields in Onion Peel Extracts by Washing (세척방법에 따른 양파껍질추출물의 Quercetin수율 및 잔류농약 제거효과)

  • Jeong, Eun-Jeong;Cha, Yong-Jun
    • Journal of Life Science
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    • v.22 no.12
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    • pp.1665-1671
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    • 2012
  • This study was conducted to assess the removal of residual pesticides and to obtain high amounts of quercetin in onion peel extracts (OPEs) by 4 washing treatments. Washing is one of the standard processing steps in obtaining functional food ingredients from onion peel. After a first detergent wash (0.2% w/v) (DW) and hot air drying ($80^{\circ}C$, 24 hr) (B), 4 washing treatments were tested, including a second DW (C), ultrasonication ($50^{\circ}C$, 10 min) plus DW (D), 0.3% $H_2O_2$ (v/v) plus DW (E), and blanching ($95-97^{\circ}C$, 2 min) plus DW (F). This was followed by 60% (v/v) ethanol extraction and vacuum freeze drying of the OPE. The E treatment yielded 89.04% OPE and a quercetin content of 96.84% in the OPE compared with the B treatment, and had the highest efficiency of all treatments tested. The OPE was tested for the presence of 177 residual pesticides and three compounds were detected in all treatments: cyhalothirn, fluquinconazole and procymidone. Cyhalothirn and fluquinconazole levels were below the permitted levels for fresh onion, while procymidone was present in the high level range of 128.01~133.46 mg/kg in all samples. The E treatment was a better washing method than the others for removal of residual pesticides. It could reduce the level of residual pesticides without changing the functional properties of the OPE.

The Effect of Intravenous Contrast on SUV Value in $^{18}F$-FDG PET/CT using Diagnostic High Energy CT (진단용 고선량 CT를 이용한 $^{18}F$-FDG PET/CT 촬영시 정맥 조영제가 SUV 값에 미치는 영향)

  • Jeong, Young-Jin;Kang, Do-Young
    • Nuclear Medicine and Molecular Imaging
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    • v.40 no.3
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    • pp.169-176
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    • 2006
  • Purpose: According to the development of CT scanner in PET/CT system, the role of CT unit as a diagnostic tool has been more important. To improve the diagnostic ability of CT scanner, it is a key aspect that CT scanning has to be performed with high dose energy and intravenous (IV) contrast. So we investigated the effect of IV contrast media on the maximum SUV (maxSUV) of normal tissues and pathologic lesions using PET/CT scanner with high dose CT scanning. Materials & Methods: The study enrolled 13 patients who required PET/CT evaluation. At first, the patients were performed whole body non-contrast CT (NCCT-120 kVp, 130 mAs) scan. Then contrast enhanced CT (CECT) scan was performed immediately. Finally PET scan was followed. The PET omission data were reconstructed twice, once with the NCCT and again with the CECT. We measured the maxSUV of 10 different body regions that were considered as normal in ail patients. Also pathologic lesions were investigated. Results: There were not seen focal artifacts in PET images based on CT with IV contrast agent. Firstly, 130 normal regions in 13 patients were evaluated. The maxSUV was significantly different between two PET images (p<0.00)). The maxSUV was $1.1{\pm}0.5$ in PET images with CECT-corrected attenuation and $1.0{\pm}0.5$ in PET images with NCCI-corrected attenuation. The limit of agreement was $0.1{\pm}0.3$ in Bland-Altman analysis. Especially there were significant differences in 6 of 10 regions, apex and base of the right lung, ascending aorta, segment 6 & segment 8 of the liver and spleen (p<0.05). Secondly, 39 pathologic lesions were evaluated. The maxSUV was significantly different between two PET images (p<0.001). The maxSUV was $4.7{\pm}2.0$ in PET images with CECT-corrected attenuation and $4.4{\pm}2.0$ in PET images with NCCT-corrected attenuation. The limit of agreement was $0.4{\pm}0.8$ in Bland-Altman analysis. Conclusion: Although there were increases of maxSUVs in the PET images based on CT with IV contrast agent, it was very narrow in the range of limit of agreement. So there was no significant effect to clinical interpretation for PET images that were corrected attenuation with high dose CT using IV contrast.

Preparation of Korean Traditional Alcoholic Beverage (Yakju) by a Protoplast Fusion Yeast Strain Utilizing Starch and its Quality Characteristics (전분분해 효모융합체를 이용한 전통 발효주의 제조와 품질특성)

  • Ju, Min-No;Hong, Sung-Wook;Kim, Kwan-Tae;Yum, Sung-Kwan;Kim, Gye-Won;Chung, Kun-Sub
    • Korean Journal of Food Science and Technology
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    • v.41 no.5
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    • pp.541-546
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    • 2009
  • The objectives of this study were to evaluate the physico-chemical and sensory characteristics of a Korean traditional alcoholic beverage (yakju) prepared using different nuruk (Korean-style koji) concentrations and yeasts such as the fusant FA776 and Saccharomyces cerevisiae KOY-1, respectively. The fusant FA776, which has alcohol-fermenting and starch-utilizing properties, was formed by Saccharomyces cerevisiae KOY-1 and Saccharomyces diastaticus KCTC1804. The fermentation trial was conducted in a 5 L lab-scale jar at $25^{\circ}C$. The maximum alcohol production of the K-100 and F-50 reached levels of 135.0 mg/mL and 119.4 mg/mL, respectively. The pH values were in a range of 4.3-4.5. Total acidity was in a range of 0.47-0.60%. Organic acids and amino acids were analyzed in order to evaluate variations in its composition and content via HPLC analysis. Organic acids including lactic acid, citric acid, malic acid, and pyruvic acid, and 16 kinds of amino acids, including aspartic acid, were detected in all treatments. K-100 showed the highest amino acid contents, whereas F-50 exhibited the lowest amino acid contents. Volatile flavor components such as phenylethyl alcohol, isoamyl alcohol, 2-methylthiophane, isobutyl alcohol, and ethyl succinate were detected as a major component in all treatments, as determined via gas chromatography. The results of our sensory evaluation demonstrated that Yakju fermented by the FA776 fusant yielded more favorable results than S. cerevisiae KOY-1.

Nonstoichiometry of the Niobium Oxide (산화니오브의 비화학양론)

  • Yo Chul Hyun;Roh Kwon Sun;Lee Sung Joo;Kim Keu Hong;Oh Eung Ju
    • Journal of the Korean Chemical Society
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    • v.35 no.4
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    • pp.329-334
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    • 1991
  • The x values and electrical conductivity of the nonstoichiometric compound NbO$_x$ have been measured in a temperature range 700$^{\circ}C$ to 1100$^{\circ}C$ under oxygen partial pressure of 2 ${\times}$ 10$^{-1}$ ∼ 1 ${\times}$ 10$^{-5}$ atm. The NbO$_x$ is a stoichiometrical compound of Nb$_2$O$_5$ under oxygen partial pressure higher than 1.0 ${\times}$ 10$^{-2}$ atm at the above temperature range. The x values were found to vary between 2.48491 and 2.49900 in a temperature range 700$^{\circ}C$ to 1100$^{\circ}C$ under oxygen partial pressure lower than 1 ${\times}$ 10$^{-3}$ atm. The enthalpy of the formation for x' in NbO$_{2.50000-x'}$(${\Delta}H_f$) increased of 15.98 to 17.26 kcal/mol under the conditions. The electrical conductivity (${\sigma}$) of the oxide varied from 10$_4$ to 10$_1$ ohm$_1$cm$_1$ in the above conditions. The activation energy for the conduction was about 1.7 eV. The oxygen pressure dependency of the conductivity (or 1/n value) was about -1/4. The nonstoichiometric conduction mechanism of the oxide has been discussed with the x' values, the ${\sigma}$ values, and the thermodynamic data.

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Synthesis and Rietveld Structure Refinement of Mn-Tourmalines (Tsilaisite) (Mn-전기석(Tsilaisite)의 합성 및 리트벨트 구조분석)

  • Grover John;Choi Jin-Beom
    • Journal of the Mineralogical Society of Korea
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    • v.19 no.1 s.47
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    • pp.15-29
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    • 2006
  • Synthetic Mn-tourmalines (tsilaisite) were obtained by hydrothermal synthesis under the condition of 2 Kbar, $375{\sim}700^{\circ}C$, and 50 day-run-time with complete substitution of Mg in dravite by Mn (Mn%=0, 25, 50, 75, and 100%). They are all 6 samples containing Mn-tourmaline with some amounts of albite, spessartine, rhodocrosite, phlogopite etc, showing different synthetic condition of temperature and Mn composition. Synthetic Mn-tourmalines are of site deficiency in X-site ($0.53{\sim}0.68$) more than that of natural ones (approx. $0.2{\sim}0.3$) and show Mn cations occupying Y-site less than expected with initial experiments, leading to failure in synthesis of end-member tsilaisite. Rietveld structural refinements reveal that $R_{wp}$ ($R_{p}/R_{exp}$) is in the range of 13.35 and 18.62%, $R_{B}$ and S (CofF) are $4.85{\sim}6.25%$ (S-18: 8.57%), $1.31{\sim}1.59$ (S-18: 1.81), respectively. Unit cell parameters (space group R3m, z=3) are ${\alpha}=15.8994\;{\AA}$ and $c=7.1846\;{\AA}$ in average (S-18: ${\alpha}=15.9491\;{\AA},\;c=7.1773\;{\AA}$). Average bond lengths of and are $2.67{\sim}2.69\;{\AA}$ (S-18: $2.65\;{\AA}$) and $2.00{\sim}2.02\;{\AA}$ (S-18: $1.96\;{\AA}$), respectively. Ditrigonality (${\delta}$) are in the range of 0.022 and 0.031 (S-18: 0.061), indicating degrading symmetry with increase of Mn content.